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GB 23200.81-2016: Food safety national standard -- Method for Detecting the Residue of West Majin in Meat and Meat Products
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Food safety national standard -- Method for Detecting the Residue of West Majin in Meat and Meat Products
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GB 23200.81-2016
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Basic data | Standard ID | GB 23200.81-2016 (GB23200.81-2016) | | Description (Translated English) | Food safety national standard -- Method for Detecting the Residue of West Majin in Meat and Meat Products | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 9,920 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN 0594-1996 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration | GB 23200.81-2016: Food safety national standard -- Method for Detecting the Residue of West Majin in Meat and Meat Products
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Food safety national standard - Method for Detecting the Residue of West Majin in Meat and Meat Products
National Standards of People's Republic of China
GB
Instead of SN 0594-1996
National standards for food safety
Method for Detecting the Residue of West Majin in Meat and Meat Products
National food safety standards-
Determination of simazine residue in meat and meat products
2016-12-18 release
2017-06-18 Implementation
National Health and Family Planning Commission of the People 's Republic of China
Issued by the Ministry of Agriculture of the People 's Republic of China
State Administration of Food and Drug Administration
Foreword
This standard replaces SN/T 0594-1996 "Test Method for Residues of West Majin in Exported Meat and Meat Products".
Compared with SN/T 0594-1996, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name and scope of the "export of meat and meat products" to "meat and meat products";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 0594-1996.
National standards for food safety
Method for Detecting the Residue of West Majin in Meat and Meat Products
1 Scope
This standard specifies the method for the determination of mesazepam residues in meat and meat products by gas chromatography.
This standard applies to the test of residual residues of beef in the beef, other food can refer to the implementation.
2 normative reference documents
The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this
file. For undated references, the latest edition (including all modifications) applies to this document.
GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs
GB/T 6682 Analytical laboratory water specifications and test methods
3 principle
The sample was extracted with a dichloromethane-methanol mixed solution and the extract was purified by a Florisil column using gas chromatography with a nitrogen and phosphorus detector
Instrument determination, external standard method quantitative.
4 reagents and materials
Unless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682.
4.1 Reagents
4.1.1 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, set the dryer in the spare.
4.1.2 Florisil. for chromatography, 100-200 mesh, at 650 ℃ for 4 h, before drying at 130 ℃ for 5 h, after cooling stored in dense
Closed container, spare.
4.2 solution preparation
4.2.1 Acetone-petroleum ether mixed solution (15 85). Take 150 mL of acetone, add 850 mL of petroleum ether and shake well.
4.2.2 Dichloromethane - methanol mixed solution (9 1). take 900 mL of dichloromethane, add 100 mL of methanol, shake back.
4.3 standards
4.3.1 Xi Ma Jin standard. purity ≥ 98%.
4.4 standard solution preparation
4.4.1 Simaxin standard solution. accurately weighed the appropriate amount of Simazine standard, with acetone prepared into 100 μg/mL standard stock solution, according to
Need to re-use acetone diluted to the appropriate concentration of standard working solution.
5 instruments and equipment
5.1 gas chromatograph, with nitrogen and phosphorus detector.
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Rotary Evaporator.
5.4 Florisil column. glass column, 40 cm horizontal1.5 cm (inner diameter), top-down filling 2 cm high anhydrous sodium sulfate, 10 g
Florisil, 2 cm high anhydrous sodium sulfate. Pre-leaching with acetone-petroleum ether mixture (15 85) before use.
5.5 Ultrasonic water bath.
6 Preparation and storage of samples
6.1 Preparation of the sample
A sample of about 1 kg was taken from all the samples taken. The sample was sampled according to GB 2763 Appendix A,
Mix, are divided into two, respectively, into the clean container as a sample. Sealed and marked.
6.2 Sample storage
The sample was stored at -18 ° C or lower.
During sample and sample preparation, the sample should be protected from contamination or changes in the residue content.
7 Analysis steps
7.1 Extraction
Weigh the sample about 30 g (accurate to 0.01 g). Add 30 g of anhydrous sodium sulfate, ground into powder, into the conical flask. Add 100 mL
Dichloromethane - methanol (9 1) mixture, ultrasonic oscillation 20 min. Filtrate with a cloth funnel to retain the filtrate. The residue was then washed with 100 mL of dichloromethane
Alkane-methanol (9 1) mixture, as described above. The filtrate was combined in a vial of rotary evaporator. And dried in a 50 ° C water bath under reduced pressure
dry.
7.2 Purification
The residue was dissolved three times with 20 mL of acetone-petroleum ether (15 85) and the solution was poured into a florite column. With 100 mL
Acetone - petroleum ether (15 85), controlled flow rate of 2-3 drops per second, and the effluent was received in an evaporating flask of rotary evaporative liquid. Water at 60 ° C
Bath in the bath to dry. With acetone to 5.0 mL, for GC determination.
7.3 Determination
7.3.1 Gas Chromatographic Reference Conditions
A) Column. HP-1.5 m0.53 mm (id), film thickness 2.65 m.
B) Column temperature. 155 ° C.
C) Inlet temperature. 240 ° C.
D) Detector temperature. 250 ° C.
E) Carrier gas. nitrogen, purity greater than or equal 99.99%, 40 mL/min.
F) Hydrogen. 2 mL/min.
G) air. 140 mL/min
H) Injection volume. 2 μL.
I) Injection method. No split injection.
7.3.2 Chromatographic determination
According to the sample solution of the content of Sima Jin, selected peak area similar to the standard working solution, the standard working solution and sample solution in the West Majin
The response value should be within the instrument detection linear range. Standard working solution and sample solution volume measurement. In the above chromatographic conditions
, The retention time of Simaxin was 2.2 min. The chromatogram of the standard sample is shown in Figure A1 in Appendix A.
7.4 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
The data processing is calculated as follows. (1)
Mhs
VCh
.. (1)
Where.
X - the residual amount of cimetidine in milligrams per milligram, mg/kg;
H - the peak height of midaximat in sample solution, mm;
V - the final volume of the sample solution, in milliliters, mL;
Hs - standard working fluid in the West Majin peak height, mm;
C - standard working solution in the concentration of cimetidine in micrograms per milliliter, g/mL;
M - the amount of sample represented by the final sample, in grams, g.
Note. The result of the calculation shall be deducted from the blank value. The result of the measurement shall be expressed as the arithmetic mean of the parallel measurement, and two valid digits shall be retained.
9 precision
9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix B requirements.
9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix C requirements.
10% limit and recovery rate
10.1 Quantitation limits
The limit of quantification of this method was 86 mg/kg.
10.2 Recovery rate
When the addition level was 0.02 mg/kg, 0.05 mg/kg and 0.1 mg/kg, the recovery of Simazine was 89.6-91.4%.
Appendix A
(Informative)
Standard chromatogram
Figure A1 Chromatogram of standards
Appendix B
(Normative appendix)
Laboratory repeatability requirements
Table B.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix C
(Normative appendix)
Inter-laboratory reproducibility requirements
Table C.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
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